JP2019167267A - Die for growing single crystal by efg method, method for growing single crystal by efg method and single crystal grown by efg method - Google Patents

Die for growing single crystal by efg method, method for growing single crystal by efg method and single crystal grown by efg method Download PDF

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JP2019167267A
JP2019167267A JP2018056165A JP2018056165A JP2019167267A JP 2019167267 A JP2019167267 A JP 2019167267A JP 2018056165 A JP2018056165 A JP 2018056165A JP 2018056165 A JP2018056165 A JP 2018056165A JP 2019167267 A JP2019167267 A JP 2019167267A
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single crystal
die
efg method
growing
efg
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JP7147213B2 (en
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克己 川崎
Katsumi Kawasaki
克己 川崎
潤 平林
Jun Hirabayashi
潤 平林
藤田 実
Minoru Fujita
実 藤田
井ノ口 大輔
Daisuke Inokuchi
大輔 井ノ口
潤 有馬
Jun Arima
潤 有馬
近藤 牧雄
Makio Kondo
牧雄 近藤
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TDK Corp
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TDK Corp
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Priority to CN201980018372.8A priority patent/CN111836920A/en
Priority to EP19771196.3A priority patent/EP3770307A4/en
Priority to PCT/JP2019/002551 priority patent/WO2019181197A1/en
Priority to US16/982,280 priority patent/US11492724B2/en
Priority to TW108109155A priority patent/TWI759587B/en
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    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/60Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • C30B29/64Flat crystals, e.g. plates, strips or discs
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B15/00Single-crystal growth by pulling from a melt, e.g. Czochralski method
    • C30B15/34Edge-defined film-fed crystal-growth using dies or slits
    • CCHEMISTRY; METALLURGY
    • C30CRYSTAL GROWTH
    • C30BSINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
    • C30B29/00Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
    • C30B29/10Inorganic compounds or compositions
    • C30B29/16Oxides

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  • Crystallography & Structural Chemistry (AREA)
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  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

To improve the uniformity of impurity concentration of a grown single crystal.SOLUTION: A die 1 for growing a single crystal by an EFG method comprises: a lower surface 2 immersed in a raw material melt 12 having added impurities; a rectangular upper surface 5 facing a seed crystal 15 and having a long side 3 and a short side 4; and a plurality of slit parts 6 extended from the lower surface 2 to the upper surface 5 and raising a raw material melt 12 from the lower surface 2 to the upper surface 5. Since the longitudinal directions 7l of the openings 7 on the upper surface 5 of the plurality of slit parts 6 are parallel to each other and are not parallel to the long side 3 of the upper surface 5, an interval δ between the openings 7 of the slit parts 6 adjacent to each other is shorter than when the longitudinal directions 7l of the openings 7 on the upper surface 5 of the slit parts 6 are parallel to the long side 3 of the upper surface 5 in the total area of the openings 7 of the slit parts 6. Since segregation of impurities between the slit parts 6 hardly occurs, the uniformity of impurity concentration of a grown single crystal 14 can be improved.SELECTED DRAWING: Figure 2

Description

本発明は、EFG法による単結晶育成用のダイ、EFG法による単結晶育成方法及びEFG法による単結晶に関する。   The present invention relates to a die for growing a single crystal by an EFG method, a method for growing a single crystal by an EFG method, and a single crystal by an EFG method.

EFG(Edge-defined Film-fed Growth)法による単結晶の育成では、育成される単結晶の育成方向に直交する断面の形状が単結晶育成用のダイの上面の形状より規定される。単結晶は、基板として薄板状に加工されて使用されることが多い。単結晶育成用のダイの上面の形状を矩形として矩形断面の単結晶を育成すると、育成後に単結晶を基板に加工する際の加工ロスを大幅に抑制することができる。このため、EFG法は様々な単結晶の育成に用いられている。   In the growth of a single crystal by an EFG (Edge-defined Film-fed Growth) method, the shape of the cross section perpendicular to the growth direction of the single crystal to be grown is defined by the shape of the upper surface of the single crystal growth die. Single crystals are often used after being processed into a thin plate shape as a substrate. When a single crystal having a rectangular cross section is grown with the shape of the upper surface of the die for growing a single crystal being a rectangle, processing loss when processing the single crystal into a substrate after the growth can be greatly suppressed. For this reason, the EFG method is used for growing various single crystals.

例えば、特許文献1では、加工ロスの低減のために、厚さ11mm以上の厚板状の単結晶育成を行い、一枚の厚板状の単結晶からスライス加工により複数の薄板状の基板を作製する方法が提案されている。特許文献1の単結晶育成用のダイでは、ダイの上面でのスリットの開口部の長手方向のそれぞれがダイの矩形の上面の長辺に対して平行である複数のスリットが設けられている。   For example, in Patent Document 1, in order to reduce processing loss, a thick plate-like single crystal having a thickness of 11 mm or more is grown, and a plurality of thin plate-like substrates are formed by slicing from a single thick plate-like single crystal. A manufacturing method has been proposed. In the die for growing a single crystal in Patent Document 1, a plurality of slits are provided in which the longitudinal direction of the opening of the slit on the upper surface of the die is parallel to the long side of the rectangular upper surface of the die.

ところで、半導体特性や蛍光特性と言った特定の特性を基板に付与する目的で、不純物が単結晶に添加されることがある。付与された特性効果を基板内で均一化するには、添加された不純物が単結晶内で均一に分布することが望ましい。しかし、非特許文献1に記載されているように、スリットからの距離に応じて育成された単結晶の不純物濃度が変動することが知られている。そこで、上記の特許文献1の技術のように複数のスリットが上面に設けられ、互いに隣接するスリットの距離を短くしたダイにより、単結晶を育成することが考えられる。   Incidentally, impurities may be added to the single crystal for the purpose of imparting specific characteristics such as semiconductor characteristics and fluorescence characteristics to the substrate. In order to make the imparted characteristic effect uniform in the substrate, it is desirable that the added impurities are uniformly distributed in the single crystal. However, as described in Non-Patent Document 1, it is known that the impurity concentration of a single crystal grown according to the distance from the slit varies. Therefore, it is conceivable to grow a single crystal by using a die having a plurality of slits provided on the upper surface and shortening the distance between adjacent slits as in the technique of Patent Document 1 described above.

特許第5891028号公報Japanese Patent No. 5891028

渡辺、他5名、「EFG法によるβ−Ga2O3単結晶のドーパント偏析」、第63回応用物理学会春季学術講演会 講演予稿集(2016 東京工業大学 大岡山キャンパス)、応用物理学会、2016年、p.12−013Watanabe et al., “Dopant segregation of β-Ga2O3 single crystal by EFG method”, 63rd JSAP Spring Meeting, 2016 (Tokyo Institute of Technology, Ookayama Campus), JSAP, 2016 p.12-013

しかしながら、上記の特許文献1のような技術では、育成された単結晶の不純物濃度の均一性が不充分であり、改善が望まれている。   However, in the technique as described in Patent Document 1 above, the uniformity of the impurity concentration of the grown single crystal is insufficient, and improvement is desired.

そこで本発明は、育成された単結晶の不純物濃度の均一性を向上させることができるEFG法による単結晶育成用のダイ、EFG法による単結晶育成方法及びEFG法による単結晶を提供することを目的とする。   Accordingly, the present invention provides a die for growing a single crystal by the EFG method, a single crystal growing method by the EFG method, and a single crystal by the EFG method that can improve the uniformity of the impurity concentration of the grown single crystal. Objective.

本発明は、EFG法による単結晶育成用のダイであって、不純物を添加された原料融液に浸漬される下面と、種結晶と対向させられ、長辺と長辺よりも短い短辺とを有する矩形状の上面と、下面から上面へと延在し、原料融液を下面から上面まで上昇させる複数のスリット部とを備え、複数のスリット部の上面での開口部の長手方向のそれぞれは互いに平行であり、上面の長辺に対して非平行であるEFG法による単結晶育成用のダイである。   The present invention is a die for growing a single crystal by the EFG method, and is a lower surface immersed in a raw material melt to which impurities are added, a seed crystal, a long side and a short side shorter than the long side. Each having a rectangular upper surface and a plurality of slit portions extending from the lower surface to the upper surface and raising the raw material melt from the lower surface to the upper surface, each in the longitudinal direction of the openings on the upper surfaces of the plurality of slit portions Are dies for single crystal growth by the EFG method which are parallel to each other and non-parallel to the long side of the upper surface.

この構成によれば、EFG法による単結晶育成用のダイにおいて、不純物を添加された原料融液に浸漬される下面と、種結晶と対向させられ、長辺と長辺よりも短い短辺とを有する矩形状の上面と、下面から上面へと延在し、原料融液を下面から上面まで上昇させる複数のスリット部とを備え、複数のスリット部の上面での開口部の長手方向のそれぞれは互いに平行であり、上面の長辺に対して非平行であるため、同じスリット部の開口部の総面積では、スリット部の上面での開口部の長手方向のそれぞれが上面の長辺に対して平行である場合よりも、互いに隣接するスリット部のそれぞれの間隔は短くなり、スリット部のそれぞれの間での不純物の偏析が生じ難くなるため、育成された単結晶の不純物濃度の均一性を向上させることができる。   According to this configuration, in the die for growing a single crystal by the EFG method, the lower surface immersed in the raw material melt to which the impurity is added, the long side and the short side shorter than the long side are opposed to the seed crystal. Each having a rectangular upper surface and a plurality of slit portions extending from the lower surface to the upper surface and raising the raw material melt from the lower surface to the upper surface, each in the longitudinal direction of the openings on the upper surfaces of the plurality of slit portions Are parallel to each other and non-parallel to the long side of the upper surface. Therefore, in the total area of the opening of the same slit, the longitudinal direction of the opening on the upper surface of the slit is relative to the long side of the upper surface. The spacing between adjacent slits is shorter than when they are parallel to each other, and segregation of impurities between the slits is less likely to occur. Can be improved .

この場合、複数のスリット部の上面での開口部の長手方向のそれぞれは、上面の短辺に対して平行であることが好適である。   In this case, each of the longitudinal directions of the openings on the upper surfaces of the plurality of slit portions is preferably parallel to the short sides of the upper surface.

この構成によれば、複数のスリット部の上面での開口部の長手方向のそれぞれは、上面の短辺に対して平行であるため、スリット部の上面での開口部の長手方向のそれぞれが上面の長辺に対して平行である場合よりも、互いに隣接するスリット部のそれぞれの間隔は短くなり、育成された単結晶の不純物濃度の均一性を向上させることができる。   According to this configuration, each of the longitudinal directions of the openings on the upper surfaces of the plurality of slit portions is parallel to the short side of the upper surface, so that each of the longitudinal directions of the openings on the upper surface of the slit portions is the upper surface. As compared with the case where the slits are parallel to the long side, the interval between the adjacent slit portions is shortened, and the uniformity of the impurity concentration of the grown single crystal can be improved.

また、複数のスリット部の中で上面の外縁部に上面での開口部が最も近接しているスリット部の上面での開口部の上面の外縁部からの距離は2mm以下であることが好適である。   Moreover, it is preferable that the distance from the outer edge part of the upper surface of the opening part in the upper surface of the slit part where the opening part on the upper surface is closest to the outer edge part of the upper surface among the plurality of slit parts is 2 mm or less. is there.

この構成によれば、複数のスリット部の中で上面の外縁部に上面での開口部が最も近接しているスリット部の上面での開口部の外縁部からの距離は2mm以下であるため、育成された単結晶の不純物濃度が均一化する領域を拡大させることができる。   According to this configuration, the distance from the outer edge portion of the opening on the upper surface of the slit portion where the opening portion on the upper surface is closest to the outer edge portion of the upper surface among the plurality of slit portions is 2 mm or less, The region where the impurity concentration of the grown single crystal becomes uniform can be enlarged.

また、互いに隣接するスリット部の上面での開口部の長手方向に沿った中心線の相互の間隔は2mm以下であることが好適である。   In addition, it is preferable that the distance between the center lines along the longitudinal direction of the opening on the upper surface of the adjacent slits is 2 mm or less.

この構成によれば、互いに隣接するスリット部の上面での開口部の長手方向に沿った中心線の相互の間隔は2mm以下であるため、育成された単結晶の不純物濃度の均一性をより向上させることができる。   According to this configuration, since the distance between the center lines along the longitudinal direction of the opening on the upper surface of the slits adjacent to each other is 2 mm or less, the uniformity of the impurity concentration of the grown single crystal is further improved. Can be made.

また、複数のスリット部の上面での開口部の短手方向の長さのそれぞれは2mm以下であることが好適である。   In addition, each of the lengths of the openings in the short direction on the upper surfaces of the plurality of slit portions is preferably 2 mm or less.

この構成によれば、複数のスリット部の上面での開口部の短手方向の長さのそれぞれは2mm以下であるため、スリット部が原料融液を下面から上面まで上昇させる高さを増加させることができる。   According to this configuration, each of the lengths in the short direction of the openings on the upper surfaces of the plurality of slit portions is 2 mm or less, so that the height at which the slit portions raise the raw material melt from the lower surface to the upper surface is increased. be able to.

一方、本発明は、上記本発明のEFG法による単結晶育成用のダイを用いたEFG法による単結晶育成方法である。   On the other hand, the present invention is a method for growing a single crystal by the EFG method using the die for growing a single crystal by the EFG method of the present invention.

この構成によれば、EFG法により不純物濃度の均一性を向上させた単結晶を育成することができる。   According to this configuration, a single crystal with improved impurity concentration uniformity can be grown by the EFG method.

また、本発明は、単結晶の育成方向に直交する断面において、断面の外縁部から1mmの距離の範囲を除いた領域における不純物濃度の変動係数が30%以下である上記本発明のEFG法による単結晶育成方法によって育成されたEFG法による単結晶である。   Further, the present invention is based on the above-described EFG method according to the present invention in which the variation coefficient of the impurity concentration in a region excluding the distance of 1 mm from the outer edge of the cross section is 30% or less in the cross section perpendicular to the growth direction of the single crystal It is a single crystal by the EFG method grown by the single crystal growth method.

この構成によれば、不純物濃度の均一性が向上され、特性がより均一化した単結晶を提供することができる。   According to this configuration, it is possible to provide a single crystal with improved uniformity of impurity concentration and more uniform characteristics.

本発明のEFG法による単結晶育成用のダイ、EFG法による単結晶育成方法及びEFG法による単結晶によれば、育成された単結晶の不純物濃度の均一性を向上させることができる。   According to the die for growing a single crystal by the EFG method of the present invention, the single crystal growing method by the EFG method, and the single crystal by the EFG method, the uniformity of the impurity concentration of the grown single crystal can be improved.

実施形態に係るEFG法による坩堝、EFG法による単結晶育成用のダイ及びEFG法による単結晶を示す斜視図である。It is a perspective view which shows the crucible by the EFG method which concerns on embodiment, the die | dye for single crystal growth by the EFG method, and the single crystal by the EFG method. 図1のEFG法による坩堝及びEFG法による単結晶育成用のダイの縦断面図である。It is a longitudinal cross-sectional view of the crucible by the EFG method of FIG. 1 and the die | dye for single crystal growth by the EFG method. 実施形態に係るEFG法による単結晶育成用のダイの平面図である。It is a top view of the die for single crystal growth by the EFG method concerning an embodiment. 従来のEFG法による単結晶育成用のダイの平面図である。It is a top view of the die | dye for single crystal growth by the conventional EFG method. 実施例に係るEFG法による単結晶育成用のダイの諸元を示す表である。It is a table | surface which shows the item of the die | dye for single crystal growth by the EFG method which concerns on an Example. 比較例に係るEFG法による単結晶育成用のダイの諸元を示す表である。It is a table | surface which shows the specification of the die | dye for single crystal growth by the EFG method which concerns on a comparative example. 実施例に係るEFG法による単結晶の不純物濃度を示すグラフである。It is a graph which shows the impurity concentration of the single crystal by the EFG method which concerns on an Example. 比較例に係るEFG法による単結晶の不純物濃度を示すグラフである。It is a graph which shows the impurity concentration of the single crystal by the EFG method which concerns on a comparative example.

以下、本発明の実施形態について図面を用いて詳細に説明する。本実施形態のEFG法による単結晶育成用のダイ及びEFG法による単結晶育成方法は、EFG法により、例えば、β−Ga単結晶の育成を行うためのものである。図1及び図2に示すように、EFG法による単結晶製造装置10は、Ga系等の原料融液12を収容する坩堝11と、坩堝11の中に設置されたEFG法による単結晶育成用のダイ1と、ダイ1の上面5を除く坩堝11の上面を覆う蓋13と、Ga系等の種結晶15を保持する種結晶保持具16と、種結晶保持具16を昇降可能に支持するシャフト17とを備える。 Hereinafter, embodiments of the present invention will be described in detail with reference to the drawings. The single crystal growth die by the EFG method and the single crystal growth method by the EFG method of the present embodiment are for growing, for example, a β-Ga 2 O 3 single crystal by the EFG method. As shown in FIGS. 1 and 2, a single crystal manufacturing apparatus 10 using an EFG method includes a crucible 11 that contains a raw material melt 12 such as a Ga 2 O 3 system, and a single crystal device that uses an EFG method installed in the crucible 11. A crystal growing die 1, a lid 13 covering the upper surface of the crucible 11 excluding the upper surface 5 of the die 1, a seed crystal holder 16 holding a seed crystal 15 such as a Ga 2 O 3 system, and a seed crystal holder 16 And a shaft 17 that supports the shaft so as to be movable up and down.

坩堝11は不図示の加熱手段により加熱され、例えば、β−Gaの融点を越える1800℃以上まで昇温させられる。坩堝11の中に収容されたSn等の添加物の添加濃度0.016mol%のGa系等の固体原料は、昇温過程で融解しGa系等の原料融液12へと変化する。坩堝11及びEFG法による単結晶育成用のダイ1は、Ga系等の原料融液12を収容し得る耐熱性を有するイリジウム系金属材料からなる。蓋13は、坩堝11からGa系等の原料融液12が蒸発することを抑制し、さらにはGa系等の種結晶15等にGa系等の原料融液12の蒸気が付着することを防ぐ。 The crucible 11 is heated by a heating means (not shown), and the temperature is raised to, for example, 1800 ° C. or higher, which exceeds the melting point of β-Ga 2 O 3 . The solid raw material such as Ga 2 O 3 and the like having an additive concentration of 0.016 mol% of the additive such as Sn contained in the crucible 11 is melted in the temperature rising process to the raw material melt 12 such as Ga 2 O 3 And change. The crucible 11 and the die 1 for growing a single crystal by the EFG method are made of a heat-resistant iridium metal material that can accommodate a raw material melt 12 such as a Ga 2 O 3 system. The lid 13 suppresses evaporation of the Ga 2 O 3 -based material melt 12 from the crucible 11, and further Ga 2 O 3 -based material melt such as a Ga 2 O 3 -based seed crystal 15. Twelve vapors are prevented from sticking.

EFG法による単結晶育成用のダイ1は、Sn等の不純物を添加されたGa系等の原料融液12に浸漬される下面2と、Ga系等の種結晶15と対向させられ、長辺3と長辺3よりも短い短辺4とを有する矩形状の上面5と、下面2から上面5へと延在し、原料融液12を下面2から上面5まで上昇させる複数のスリット部6とを備える。なお、矩形状の上面5とは、例えば、上面5の長辺3と短辺4とによる角部が厳密な90°の角度以外の角度をなすものや、角部が丸みを帯びているものも含まれる。 A die 1 for growing a single crystal by the EFG method includes a lower surface 2 immersed in a raw material melt 12 such as Ga 2 O 3 to which impurities such as Sn are added, a seed crystal 15 such as Ga 2 O 3 and the like. A rectangular upper surface 5 having a long side 3 and a short side 4 shorter than the long side 3, opposed to each other, extends from the lower surface 2 to the upper surface 5, and the raw material melt 12 is raised from the lower surface 2 to the upper surface 5. And a plurality of slit portions 6 to be operated. In addition, the rectangular upper surface 5 is, for example, one in which the corners of the long side 3 and the short side 4 of the upper surface 5 form an angle other than a strict 90 ° angle, or the corners are rounded. Is also included.

図1、図2及び図3に示すように、複数のスリット部6の上面5での開口部7は長手方向7lと短手方向7sとを有する矩形状である。複数のスリット部6の上面5での開口部7の長手方向7lのそれぞれは互いに平行であり、上面5の長辺3に対して非平行である。具体的には、複数のスリット部6の上面5での開口部7の長手方向7lのそれぞれは、上面5の短辺4に対して平行である。なお、開口部7が矩形状とは、例えば、開口部7の長手方向7lと短手方向7sとによる角部が厳密な90°の角度以外の角度をなすものや、角部が丸みを帯びているものも含まれる。   As shown in FIGS. 1, 2, and 3, the opening 7 in the upper surface 5 of the plurality of slit portions 6 has a rectangular shape having a longitudinal direction 7 l and a short direction 7 s. Each of the longitudinal directions 7 l of the openings 7 on the upper surface 5 of the plurality of slit portions 6 is parallel to each other and non-parallel to the long side 3 of the upper surface 5. Specifically, each of the longitudinal directions 7 l of the openings 7 on the upper surface 5 of the plurality of slit portions 6 is parallel to the short side 4 of the upper surface 5. In addition, the opening 7 is rectangular, for example, the corner formed by the longitudinal direction 7 l and the short direction 7 s of the opening 7 forms an angle other than a strict 90 ° angle, or the corner is rounded. Is also included.

図3に示すように、複数のスリット部6の中で上面5の外縁部5eに上面5での開口部7が最も近接しているスリット部6の上面5での開口部7の上面5の外縁部5eからの距離αは2mm以下である。互いに隣接するスリット部6の上面5での開口部7の長手方向7lに沿った中心線7cの相互の間隔βのそれぞれは等しく、且つ2mm以下である。複数のスリット部6の上面5での開口部7の短手方向7sの長さγのそれぞれは2mm以下である。互いに隣接するスリット部6の上面5での開口部7の相互の間隔δのそれぞれは等しく、且つ2mm以下である。なお、スリット部6の開口部7の間隔β及び間隔δのそれぞれは必ずしも等しくなくともよい。   As shown in FIG. 3, among the plurality of slit portions 6, the opening 7 on the upper surface 5 is closest to the outer edge portion 5 e of the upper surface 5. The distance α from the outer edge portion 5e is 2 mm or less. The mutual intervals β of the center lines 7c along the longitudinal direction 7l of the opening 7 on the upper surface 5 of the slit portions 6 adjacent to each other are equal and 2 mm or less. Each of the length γ in the short direction 7 s of the opening 7 on the upper surface 5 of the plurality of slit portions 6 is 2 mm or less. The distances δ between the openings 7 on the upper surface 5 of the slits 6 adjacent to each other are equal and 2 mm or less. Note that the intervals β and δ of the openings 7 of the slit portion 6 are not necessarily equal.

以下、本実施形態のEFG法による単結晶育成用のダイ1を用いたEFG法による単結晶育成方法について説明する。図2に示すように、単結晶育成用のダイ1は、ダイ1の下面2が、坩堝11に収容され、Sn等の不純物を添加されたGa系等の原料融液12に浸漬するように坩堝11の中に設置される。Ga系等の原料融液12は、毛細管現象によりスリット部6の内部を上昇し、ダイ1の上面5に達する。 Hereinafter, a method for growing a single crystal by the EFG method using the die 1 for growing a single crystal by the EFG method of the present embodiment will be described. As shown in FIG. 2, the die 1 for growing a single crystal is immersed in a raw material melt 12 such as a Ga 2 O 3 system in which a lower surface 2 of the die 1 is housed in a crucible 11 and an impurity such as Sn is added. It is installed in the crucible 11 as described above. A raw material melt 12 such as a Ga 2 O 3 system ascends inside the slit portion 6 by capillary action and reaches the upper surface 5 of the die 1.

ダイ1の上面5が育成に適した温度になるよう不図示の加熱手段の出力調整が行われる。図1に示すように、シャフト17が下降させられ、種結晶保持具16に保持されたGa系等の種結晶15とダイ1の上面5に達したGa系等の原料融液12とが接触させられる。シャフト17が上昇させられ、Ga系等の原料融液12と接触したGa系等の種結晶15を引き上げることにより、ダイ1の上面5から育成方向Dに沿ってGa系等の単結晶14が成長する。 Output adjustment of a heating means (not shown) is performed so that the upper surface 5 of the die 1 has a temperature suitable for growth. As shown in FIG. 1, the shaft 17 is lowered and the seed crystal 15 such as Ga 2 O 3 system held by the seed crystal holder 16 and the raw material such as Ga 2 O 3 system reaching the upper surface 5 of the die 1. The melt 12 is brought into contact. Shaft 17 is raised, by pulling the seed crystal 15 of Ga 2 O 3 system or the like in contact with the raw material melt 12 of Ga 2 O 3 system, etc., along the upper surface 5 of the die 1 in the development direction D Ga 2 A single crystal 14 such as an O 3 system grows.

上記の本実施形態のEFG法による単結晶育成用のダイ1を用いたEFG法による単結晶育成方法により、例えば、単結晶14の育成方向Dに直交する断面において、断面の外縁部から1mmの距離の範囲を除いた領域における不純物濃度の変動係数が30%以下であるEFG法による単結晶14が育成される。   By the single crystal growth method by the EFG method using the die 1 for single crystal growth by the EFG method of the present embodiment described above, for example, in the cross section orthogonal to the growth direction D of the single crystal 14, 1 mm from the outer edge of the cross section The single crystal 14 is grown by the EFG method in which the variation coefficient of the impurity concentration in the region excluding the distance range is 30% or less.

本実施形態によれば、EFG法による単結晶育成用のダイ1において、不純物を添加された原料融液12に浸漬される下面2と、種結晶15と対向させられ、長辺3と長辺3よりも短い短辺4とを有する矩形状の上面5と、下面2から上面5へと延在し、原料融液12を下面2から上面5まで上昇させる複数のスリット部6とを備え、複数のスリット部6の上面5での開口部7の長手方向7lのそれぞれは互いに平行であり、上面5の長辺3に対して非平行であるため、同じスリット部6の開口部7の総面積では、スリット部6の上面5での開口部7の長手方向7lのそれぞれが上面5の長辺3に対して平行である場合よりも、互いに隣接するスリット部6の開口部7のそれぞれの間隔δは短くなり、スリット部6のそれぞれの間での不純物の偏析が生じ難くなるため、育成された単結晶14の不純物濃度の均一性を向上させることができる。   According to the present embodiment, in the die 1 for growing a single crystal by the EFG method, the lower surface 2 immersed in the raw material melt 12 to which the impurity is added is opposed to the seed crystal 15, and the long side 3 and the long side A rectangular upper surface 5 having a short side 4 shorter than 3, and a plurality of slit portions 6 extending from the lower surface 2 to the upper surface 5 and raising the raw material melt 12 from the lower surface 2 to the upper surface 5, Since each of the longitudinal directions 7 l of the openings 7 on the upper surface 5 of the plurality of slit portions 6 is parallel to each other and not parallel to the long side 3 of the upper surface 5, the total of the openings 7 of the same slit portion 6 is the same. In terms of area, each of the opening portions 7 of the slit portions 6 adjacent to each other is more than in the case where each of the longitudinal directions 7 l of the opening portion 7 on the upper surface 5 of the slit portion 6 is parallel to the long side 3 of the upper surface 5. The interval δ is shortened, and impurities between the slit portions 6 are present. Since segregation hardly occurs, it is possible to improve the uniformity of the impurity concentration in the single crystal 14 is grown.

また、本実施形態によれば、複数のスリット部6の上面5での開口部7の長手方向7lのそれぞれは、上面5の短辺4に対して平行であるため、スリット部6の上面5での開口部7の長手方向7lのそれぞれが上面5の長辺3に対して平行である場合よりも、互いに隣接するスリット部6の開口部7のそれぞれの間隔δは短くなり、育成された単結晶14の不純物濃度の均一性を向上させることができる。さらに、スリット部6の上面5での開口部7の長手方向7lのそれぞれが上面5の長辺3に対して平行である場合よりも、スリット部6の上面5での開口部7の長手方向7lの長さが短くなるため、ダイ1がより変形し難く、ダイ1の耐久性を向上させることができる。   In addition, according to the present embodiment, each of the longitudinal directions 7 l of the openings 7 on the upper surfaces 5 of the plurality of slit portions 6 is parallel to the short side 4 of the upper surface 5. The distance δ between the openings 7 of the slits 6 adjacent to each other is shorter than that in the case where each of the longitudinal directions 7 l of the openings 7 is parallel to the long side 3 of the upper surface 5. The uniformity of the impurity concentration of the single crystal 14 can be improved. Furthermore, the longitudinal direction of the opening 7 on the upper surface 5 of the slit 6 is greater than the case where each of the longitudinal directions 7 l of the opening 7 on the upper surface 5 of the slit 6 is parallel to the long side 3 of the upper surface 5. Since the length of 7 l is shortened, the die 1 is more difficult to deform and the durability of the die 1 can be improved.

また、本実施形態によれば、複数のスリット部6の中で上面5の外縁部5eに上面5での開口部7が最も近接しているスリット部6の上面5での開口部7の外縁部5eからの距離αは2mm以下であるため、育成された単結晶14の不純物濃度が均一化する領域を拡大させることができる。   In addition, according to the present embodiment, the outer edge of the opening 7 on the upper surface 5 of the slit 6 where the opening 7 on the upper surface 5 is closest to the outer edge 5 e of the upper surface 5 among the plurality of slits 6. Since the distance α from the portion 5e is 2 mm or less, the region where the impurity concentration of the grown single crystal 14 becomes uniform can be enlarged.

例えば、特許文献1の段落(0006)に記載されているように、ダイの上面での複数のスリットの開口部の長手方向のそれぞれがダイの矩形の上面の長辺に対して平行である従来の技術では、ダイを構成する板材の板厚が1mm以下だと反りが発生し、精度よくダイを製造するには2.4mm以上の板厚の板材が必要である。つまり、従来の技術では、ダイの上面の長辺に平行な方向の長い距離に亘って延在するダイの最も広い側面を構成する板材は、ダイの上面の短辺の側における両端の二箇所のみで支持されているため、ダイの機械的強度が低く、板材の板厚を厚くする必要がある。そのため従来の技術では、距離αを2mm以下とすることは困難である。   For example, as described in paragraph (0006) of Patent Document 1, each of the longitudinal directions of the openings of the plurality of slits on the upper surface of the die is parallel to the long side of the upper surface of the rectangular rectangle of the die. In this technique, warping occurs when the thickness of the plate material constituting the die is 1 mm or less, and a plate material having a thickness of 2.4 mm or more is required to manufacture the die with high accuracy. In other words, in the prior art, the plate material constituting the widest side surface of the die extending over a long distance in the direction parallel to the long side of the upper surface of the die has two locations on both ends on the short side of the upper surface of the die. Therefore, it is necessary to increase the plate thickness of the plate material because the mechanical strength of the die is low. Therefore, with the conventional technology, it is difficult to set the distance α to 2 mm or less.

一方、本実施形態では、ダイ1の上面5の長辺3に平行な方向の長い距離に亘って延在するダイ1の最も広い側面を構成する板材は、ダイ1の短辺4の側における両端の二箇所の他に、スリット部6のそれぞれを仕切る板材によっても支持される。つまり、本実施形態では、ダイ1の最も広い側面を構成する板材の支持点が多く且つ支持点がダイ1の全体に分散しているため、ダイ1の全体の機械的な強度が向上し、薄い板厚の板材でもダイ1を精度良く製造することができる。   On the other hand, in the present embodiment, the plate material constituting the widest side surface of the die 1 extending over a long distance in the direction parallel to the long side 3 of the upper surface 5 of the die 1 is on the short side 4 side of the die 1. In addition to the two places at both ends, the slit portion 6 is also supported by a plate material that partitions each of the slit portions 6. That is, in this embodiment, since the support points of the plate material constituting the widest side surface of the die 1 are many and the support points are dispersed throughout the die 1, the overall mechanical strength of the die 1 is improved. The die 1 can be accurately manufactured even with a thin plate material.

また、本実施形態によれば、互いに隣接するスリット部6の上面5での開口部7の長手方向7lに沿った中心線7cの相互の間隔βは2mm以下であるため、育成された単結晶14の不純物濃度の均一性をより向上させることができる。   Further, according to the present embodiment, since the mutual interval β of the center lines 7c along the longitudinal direction 7l of the opening 7 on the upper surface 5 of the slits 6 adjacent to each other is 2 mm or less, the grown single crystal The uniformity of the impurity concentration of 14 can be further improved.

スリット部のそれぞれを仕切る板材についても、特許文献1に記載されているような従来の技術では、スリット部のそれぞれを仕切る板材は、ダイの上面の短辺の側における両端の二箇所のみで支持され、ダイの上面の長辺に平行な方向の長い距離に亘って延在するため、スリット部のそれぞれを仕切る板材に反りが発生した場合の影響が大きく、反りを防ぐために板材の板厚を厚くする必要がある。そのため従来の技術では、間隔βを2mm以下とすることは困難である。   With regard to the plate material that partitions each of the slit portions, in the conventional technology as described in Patent Document 1, the plate material that partitions each of the slit portions is supported only at two locations on both sides of the short side of the upper surface of the die. Since it extends over a long distance in a direction parallel to the long side of the upper surface of the die, the effect of warping on the plate material that partitions each of the slit portions is large, and the plate thickness of the plate material is set to prevent warpage. It needs to be thick. Therefore, with the conventional technique, it is difficult to set the interval β to 2 mm or less.

一方、本実施形態では、ダイ1の上面5の長辺3の側において、スリット部6のそれぞれを仕切る板材が支持される板材の両端の二箇所の距離が、従来のダイ1の上面5の長辺3に平行な方向の距離よりも短い短辺4に平行な方向の距離となるため、同じ曲率半径の反りが発生したとしても、その影響が軽微となり、スリット部6のそれぞれを仕切る板材の板厚を薄くすることが可能となる。   On the other hand, in this embodiment, on the long side 3 side of the upper surface 5 of the die 1, the distance between the two ends of the plate material on which the plate material that partitions each of the slit portions 6 is supported is the distance between the upper surface 5 of the conventional die 1. Since the distance in the direction parallel to the short side 4 is shorter than the distance in the direction parallel to the long side 3, even if the curvature of the same curvature radius occurs, the influence is slight, and the plate material that partitions each of the slit portions 6 It is possible to reduce the plate thickness.

また、本実施形態によれば、複数のスリット部6の上面5での開口部7の短手方向7sの長さγのそれぞれは2mm以下であるため、スリット部6が原料融液12を下面2から上面5まで上昇させる高さを増加させることができる。   In addition, according to the present embodiment, each of the lengths γ in the short direction 7 s of the openings 7 on the upper surfaces 5 of the plurality of slit portions 6 is 2 mm or less, so that the slit portions 6 lower the raw material melt 12 on the lower surface. The height to be raised from 2 to the upper surface 5 can be increased.

また、本実施形態によれば、EFG法により不純物濃度の均一性を向上させた単結晶14を育成することができる。また、本実施形態によれば、不純物濃度の均一性が向上され、特性がより均一化した単結晶14を提供することができる。   Further, according to the present embodiment, the single crystal 14 with improved impurity concentration uniformity can be grown by the EFG method. Further, according to the present embodiment, it is possible to provide the single crystal 14 with improved uniformity of impurity concentration and more uniform characteristics.

以上、本発明の実施形態について説明したが、本発明は上記実施形態に限定されることなく様々な形態で実施される。例えば、複数のスリット部6の上面5での開口部7の形状及び配置は適宜変更され得る。   As mentioned above, although embodiment of this invention was described, this invention is implemented in various forms, without being limited to the said embodiment. For example, the shape and arrangement of the openings 7 on the upper surface 5 of the plurality of slit portions 6 can be changed as appropriate.

(実施例)
上述したEFG法による単結晶製造装置10及びEFG法による単結晶育成用のダイ1を用いて、不純物としてSnを添加されたGa系の単結晶14の育成が行われた。ダイ1の各部位の寸法又は数量は図5に示した通りである。単結晶育成用のダイ1に形成された複数のスリット部6により上昇させられたGa系の原料融液12は一体となってダイ1の上面5に拡がり、直胴部分の断面形状が幅約57mm、厚さ約18mm、直胴部分の長さが約112mmとなる厚板状のGa系の単結晶14が成長した。
(Example)
The Ga 2 O 3 -based single crystal 14 to which Sn was added as an impurity was grown using the above-described single crystal manufacturing apparatus 10 by the EFG method and the die 1 for single crystal growth by the EFG method. The size or quantity of each part of the die 1 is as shown in FIG. The Ga 2 O 3 -based material melt 12 raised by the plurality of slit portions 6 formed in the single crystal growth die 1 is spread integrally on the upper surface 5 of the die 1, and the cross-sectional shape of the straight body portion A thick plate-like Ga 2 O 3 -based single crystal 14 having a width of about 57 mm, a thickness of about 18 mm, and a length of the straight body portion of about 112 mm grew.

成長した単結晶14から直胴部分が切り出され、長さ方向(育成方向D)に交差する断面で二分割された後、得られた厚さ約18mmの2つの単結晶ブロックのそれぞれがマルチソーによる切断面が結晶主面と平行となるように18枚の平板に切断された。2つの単結晶ブロックのそれぞれが18枚の平板に切断された後、さらに平板のそれぞれの両面が研磨加工され、厚さ0.4mmの単結晶基板が一つの単結晶14から36枚作製された。   A straight body portion is cut out from the grown single crystal 14 and divided into two cross sections intersecting in the length direction (growing direction D), and each of the obtained two single crystal blocks having a thickness of about 18 mm is formed by a multi-saw. The plate was cut into 18 flat plates so that the cut surface was parallel to the crystal main surface. After each of the two single crystal blocks was cut into 18 flat plates, both sides of each flat plate were further polished to produce 36 single-crystal substrates having a thickness of 0.4 mm from 14 single crystals. .

得られた36枚の単結晶基板のうち、単結晶育成時に最も単結晶14の外側に位置し、結晶性の低い4枚を除いた32枚の単結晶基板中のSn濃度がSIMS(Secondary IonMass Spectrometry、二次イオン質量分析法)により測定された。つまり、単結晶14の育成方向Dに直交する断面において、断面の外縁部から1mmの距離の範囲を除いた領域の不純物であるSn濃度が測定された。測定結果を図7に示す。図7のグラフの横軸は、厚板状に育成したGa系の単結晶14を結晶主面と平行に切断して得た単結晶基板の厚さ方向の順番を示す。図7のグラフの縦軸は、32枚の単結晶基板のSn濃度の各測定値を基板32枚のSn濃度の平均値で除した値を示す。32枚の単結晶基板の変動係数(Cv)、即ちSn濃度の標準偏差を平均値で割った値は30%以下の12.1%であった。つまり、実施例のダイ1により育成された単結晶14の不純物濃度の均一性が高いことが判る。 Of the obtained 36 single crystal substrates, the Sn concentration in 32 single crystal substrates except for the four low crystallinity substrates located outside the single crystal 14 at the time of single crystal growth was SIMS (Secondary Ion Mass). Spectrometry, secondary ion mass spectrometry). That is, in the cross section orthogonal to the growth direction D of the single crystal 14, the Sn concentration as the impurity in the region excluding the range of the distance of 1 mm from the outer edge of the cross section was measured. The measurement results are shown in FIG. The horizontal axis of the graph in FIG. 7 indicates the order in the thickness direction of the single crystal substrate obtained by cutting the Ga 2 O 3 single crystal 14 grown in a thick plate shape in parallel with the crystal main surface. The vertical axis of the graph in FIG. 7 indicates a value obtained by dividing each measured value of the Sn concentration of 32 single crystal substrates by the average value of the Sn concentration of 32 substrates. The coefficient of variation (Cv) of 32 single crystal substrates, that is, the value obtained by dividing the standard deviation of the Sn concentration by the average value was 12.1%, which is 30% or less. That is, it can be seen that the uniformity of the impurity concentration of the single crystal 14 grown by the die 1 of the example is high.

また上記の単結晶14の育成を12回以上繰り返して行われたが、単結晶育成用のダイ1の形状に顕著な変化は認められなかった。つまり、単結晶育成用のダイ1は変形し難く、耐久性にも優れることが判る。   Further, the above-described growth of the single crystal 14 was repeated 12 times or more, but no significant change was observed in the shape of the single crystal growth die 1. That is, it can be seen that the single crystal growing die 1 is not easily deformed and has excellent durability.

(比較例)
比較例として用いた単結晶育成用のダイ20の平面図を図4に示す。ダイ20では、複数のスリット部6の上面5での開口部7の長手方向7lのそれぞれは、上面5の長辺3に対して平行である。スリット部6の開口部7の間隔β及び間隔δのそれぞれは等しい。ダイ20の各部位の寸法又は数量は図6に示した通りである。単結晶育成用のダイ20以外は、実施例と全く同じ条件で単結晶14の育成が行われ、一つの単結晶から最終的に厚さ0.4mmに研磨した単結晶基板が36枚作製された。
(Comparative example)
A plan view of a die 20 for growing a single crystal used as a comparative example is shown in FIG. In the die 20, each of the longitudinal directions 7 l of the openings 7 on the upper surface 5 of the plurality of slit portions 6 is parallel to the long side 3 of the upper surface 5. Each of the interval β and the interval δ of the opening 7 of the slit portion 6 is equal. The size or quantity of each part of the die 20 is as shown in FIG. Except for the single crystal growth die 20, the single crystal 14 is grown under exactly the same conditions as in the embodiment, and 36 single crystal substrates polished to a thickness of 0.4 mm from one single crystal are produced. It was.

得られた36枚の単結晶基板のうち、単結晶育成時に最も単結晶14の外側に位置し、結晶性の低い4枚を除いた32枚の単結晶基板中のSn濃度がSIMSにより測定された。つまり、単結晶14の育成方向Dに直交する断面において、断面の外縁部から1mmの距離の範囲を除いた領域の不純物であるSn濃度が測定された。測定結果を図8に示す。図8のグラフの横軸は、厚板状に育成したGa系の単結晶14を結晶主面と平行に切断して得た単結晶基板の厚さ方向の順番を示す。図8のグラフの縦軸は、32枚の単結晶基板のSn濃度の各測定値を基板32枚のSn濃度の平均値で除した値を示す。32枚の単結晶基板の変動係数(Cv)、即ちSn濃度の標準偏差を平均値で割った値は30%を超える35.5%であった。つまり、比較例のダイ20により育成された単結晶14の不純物濃度の均一性は低いことが判る。 Among the obtained 36 single crystal substrates, the Sn concentration in 32 single crystal substrates, which was located most outside the single crystal 14 during single crystal growth and excluding the four low crystallinity substrates, was measured by SIMS. It was. That is, in the cross section orthogonal to the growth direction D of the single crystal 14, the Sn concentration as the impurity in the region excluding the range of the distance of 1 mm from the outer edge of the cross section was measured. The measurement results are shown in FIG. The horizontal axis of the graph in FIG. 8 indicates the order in the thickness direction of the single crystal substrate obtained by cutting the Ga 2 O 3 -based single crystal 14 grown in a thick plate shape in parallel with the crystal main surface. The vertical axis of the graph in FIG. 8 represents a value obtained by dividing each measured value of the Sn concentration of 32 single crystal substrates by the average value of the Sn concentration of 32 substrates. The coefficient of variation (Cv) of 32 single crystal substrates, that is, the value obtained by dividing the standard deviation of the Sn concentration by the average value was 35.5% exceeding 30%. That is, it can be seen that the uniformity of the impurity concentration of the single crystal 14 grown by the comparative example die 20 is low.

上記の単結晶14の育成が6回繰り返えされた時点から、単結晶育成用のダイ20の上面5の中腹部に歪みが認められ、9回目以降、外側に位置するスリット部6の開口部7において、スリット部6の中央から供給されるGa系の原料融液12の量が減少し、ダイ20の上面5の全体にGa系の原料融液12が濡れ拡がらない状態となった。つまり、従来の単結晶育成用のダイ20は変形し易く、実施例のダイ1に比べて耐久性で劣ることが判る。 From the time when the growth of the single crystal 14 is repeated six times, distortion is recognized in the middle part of the upper surface 5 of the die 20 for single crystal growth, and after the ninth time, the opening of the slit portion 6 located on the outside is observed. In the portion 7, the amount of the Ga 2 O 3 -based material melt 12 supplied from the center of the slit portion 6 decreases, and the Ga 2 O 3 -based material melt 12 wets and spreads over the entire upper surface 5 of the die 20. It became a state that does not peel off. That is, it can be seen that the conventional single crystal growing die 20 is easily deformed and is inferior in durability to the die 1 of the embodiment.

1…ダイ、2…下面、3…長辺、4…短辺、5…上面、5e…外縁部、6…スリット部、7…開口部、7l…長手方向、7s…短手方向、7c…中心線、10…単結晶製造装置、11…坩堝、12…原料融液、13…蓋、14…単結晶、15…種結晶、16…種結晶保持具、17…シャフト、20…ダイ、D…育成方向、α…距離、β…間隔、γ…長さ、δ…間隔。   DESCRIPTION OF SYMBOLS 1 ... Die, 2 ... Lower surface, 3 ... Long side, 4 ... Short side, 5 ... Upper surface, 5e ... Outer edge part, 6 ... Slit part, 7 ... Opening part, 7l ... Longitudinal direction, 7s ... Short side direction, 7c ... Center line, 10 ... single crystal production apparatus, 11 ... crucible, 12 ... raw material melt, 13 ... lid, 14 ... single crystal, 15 ... seed crystal, 16 ... seed crystal holder, 17 ... shaft, 20 ... die, D ... Growth direction, α ... distance, β ... interval, γ ... length, δ ... interval.

Claims (7)

EFG法による単結晶育成用のダイであって、
不純物を添加された原料融液に浸漬される下面と、
種結晶と対向させられ、長辺と前記長辺よりも短い短辺とを有する矩形状の上面と、
前記下面から前記上面へと延在し、前記原料融液を前記下面から前記上面まで上昇させる複数のスリット部と、
を備え、
複数の前記スリット部の前記上面での開口部の長手方向のそれぞれは互いに平行であり、前記上面の前記長辺に対して非平行である、EFG法による単結晶育成用のダイ。
A die for growing a single crystal by the EFG method,
A lower surface immersed in a raw material melt to which impurities are added;
A rectangular upper surface facing the seed crystal and having a long side and a short side shorter than the long side;
A plurality of slit portions extending from the lower surface to the upper surface and raising the raw material melt from the lower surface to the upper surface;
With
A die for growing a single crystal by an EFG method, wherein the longitudinal directions of the openings on the upper surface of the plurality of slit portions are parallel to each other and non-parallel to the long side of the upper surface.
複数の前記スリット部の前記上面での前記開口部の前記長手方向のそれぞれは、前記上面の前記短辺に対して平行である、請求項1に記載のEFG法による単結晶育成用のダイ。   2. The die for growing a single crystal by the EFG method according to claim 1, wherein each of the longitudinal directions of the openings on the upper surface of the plurality of slit portions is parallel to the short side of the upper surface. 複数の前記スリット部の中で前記上面の外縁部に前記上面での前記開口部が最も近接している前記スリット部の前記上面での前記開口部の前記上面の外縁部からの距離は2mm以下である、請求項1又は2に記載のEFG法による単結晶育成用のダイ。   The distance from the outer edge of the upper surface of the opening at the upper surface of the slit portion where the opening at the upper surface is closest to the outer edge of the upper surface among the plurality of slit portions is 2 mm or less. A die for growing a single crystal by the EFG method according to claim 1 or 2. 互いに隣接する前記スリット部の前記上面での前記開口部の前記長手方向に沿った中心線の相互の間隔は2mm以下である、請求項1〜3のいずれか1項に記載のEFG法による単結晶育成用のダイ。   4. The EFG method according to claim 1, wherein an interval between center lines along the longitudinal direction of the opening on the upper surface of the slit portions adjacent to each other is 2 mm or less. 5. Dies for crystal growth. 複数の前記スリット部の前記上面での前記開口部の短手方向の長さのそれぞれは2mm以下である、請求項1〜4のいずれか1項に記載のEFG法による単結晶育成用のダイ。   The die for growing a single crystal by the EFG method according to any one of claims 1 to 4, wherein each of the lengths in the short direction of the openings on the upper surface of the plurality of slit portions is 2 mm or less. . 請求項1〜5のいずれか1項に記載のEFG法による単結晶育成用のダイを用いたEFG法による単結晶育成方法。   The single crystal growth method by the EFG method using the die | dye for single crystal growth by the EFG method of any one of Claims 1-5. 単結晶の育成方向に直交する断面において、前記断面の外縁部から1mmの距離の範囲を除いた領域における不純物濃度の変動係数が30%以下である、請求項6に記載のEFG法による単結晶育成方法によって育成されたEFG法による単結晶。   The single crystal according to the EFG method according to claim 6, wherein, in a cross section orthogonal to the growth direction of the single crystal, a coefficient of variation of an impurity concentration in a region excluding a range of a distance of 1 mm from an outer edge of the cross section is 30% or less. Single crystal by EFG method grown by the growing method.
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